Hydrazine hydrate (1:1) → 4-Isopropyl-1H-pyrazole-3,5-diamine

HRID 1912914ノート

反応式

HRID 1912914 の反応式
O.[NH2:2][NH2:3].[CH:4]([CH:7]([C:10]#[N:11])[C:8]#[N:9])([CH3:6])[CH3:5]>CCO>[CH:4]([C:7]1[C:10]([NH2:11])=[N:2][NH:3][C:8]=1[NH2:9])([CH3:6])[CH3:5]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 13180929(Propan-2-yl)propanedinitrile

生成物 1

HCID 687569004-Isopropyl-1H-pyrazole-3,5-diamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

Hydrazine monohydrate (2.05 mL, 42 mmol) was added to a solution of the product from Example 112A (1.16 g, 10.7 mmol) in EtOH (15 mL). The reaction flask was evacuated and purged with nitrogen (3 cycles), then heated at 80° C. for 22 hours. The yellow solution was cooled to room temperature and concentrated under vacuum. Toluene (8 mL) was added to the residue, and the mixture was concentrated under vacuum to remove excess hydrazine (repeated twice more) to provide the title compound. MS (ESI) m/z 141 (M+H)+.

後処理

  1. customThe reaction flask was evacuated
  2. custompurged with nitrogen (3 cycles)
  3. temperatureThe yellow solution was cooled to room temperature
  4. concentrationconcentrated under vacuum
  5. additionToluene (8 mL) was added to the residue
  6. concentrationthe mixture was concentrated under vacuum
  7. customto remove excess hydrazine (

出典と根拠

ORDレコード
ord-a62d8b2e19bd4e3d8b80a5662923c270
出典データセット
uspto-grants-2013_12
特許番号
US08609669B2

反応ノート

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